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Garcinuño Martínez, Rosa Mª

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Garcinuño Martínez
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2009 - 200912010 - 201952020 - 202415
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Mostrando 1 - 10 de 21
  • Miniatura
    Publicación
    Methacrylic acid-ethylene glycol dimethacrylate polymeric sorbent for the removal of estrogens from water
    (['Estrogens', 'Removal', 'Polymer', 'Sorbent', 'Waters', 'Balaban Publishers – Desalination Publications'], 2018-11) Gallego, Alejandrina; Bravo Yagüe, Juan Carlos; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    The presence of estrogens in environmental waters can cause adverse effects to aquatic organisms. In the last years, diverse researches have been focussed on the development of cost-effective methods for the removal of these compounds in water. In this paper, a series of methacrylic acid-ethylene glycol dimethacrylate polymers with different monomers ratio were synthesised by photochemical (UV irradiation at 365 nm) or thermal (oven at 60°C) initiation. Batch and continuous flow experiments were carried out to evaluate the capacity of these polymers to adsorb estradiol (E2), ethinylestradiol (EE2) and dienestrol (DEN). Adsorption isotherm studies revealed that Langmuir isotherm model was fitted with a better correlation than Freundlich isotherm. Finally, continuous flow experiments were carried out by microcolumn studies to check the suitability of the polymeric sorbent for the removal of estrogens from real water samples. When continuous removal experiments at 8 mL min–1 flow rate were carried out, breakthrough adsorption capacities of 28.5, 38 and 69.7 mg g–1 for E2, EE2 and DEN, respectively, were achieved.
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    Assessment of molecularly imprinted polymers as selective solid-phase extraction sorbents for the detection of cloxacillin in drinking and river water
    (MDPI, 2023-11-03) Collado, Eduardo José; Paniagua González, Gema; Bravo Yagüe, Juan Carlos; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    This paper describes a new methodology for carrying out quantitative extraction of cloxacillin from drinking and river water samples using a molecularly imprinted polymer (MIP) as a selective sorbent for solid-phase extraction (MISPE). Several polymers were synthesized via thermal polymerization using cloxacillin as a template, methacrylic acid (MAA) as a functional monomer, ethyleneglycoldimethacrylate (EGDMA) as a cross-linker and different solvents as porogens. Binding characteristics of the adequate molecularly imprinted and non-imprinted (NIP) polymers were evaluated via batch adsorption assays following the Langmuir and Freundlich isotherms and Scatchard assays. The parameters related to the extraction approach were studied to select the most appropriate polymer for cloxacillin determination. Using the optimized MIP as the SPE sorbent, a simple sample treatment methodology was combined with high-performance liquid chromatography (HPLC) to analyze cloxacillin residues in drinking and river water. Under the optimum experimental conditions, the MISPE methodology was validated using spiked samples. The linearity for cloxacillin was assessed within the limits of 0.05–1.5 g L􀀀1 and the recovery percentage was higher than 98% (RSD < 4%). The limits of detection and limits of quantification were 0.29 and 0.37 g L􀀀1 and 0.8 and 0.98 g L􀀀1 for drinking and river water, respectively. The selectivity of MIP against other ß-lactam antibiotics with similar structures (oxacillin, cefazoline, amoxicillin and penicillin V) was studied, obtaining a good recovery higher than 85% for all except cefazoline. The proposed MISPE-HPLC methodology was successfully applied for the detection of cloxacillin in drinking water from Canal de Isabel II (Madrid) and river water from the Manzanares River (Madrid).
  • Miniatura
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    Evaluation of total phenol pollution in water of San Martin Canal from Santiago del Estero, Argentina.
    (Elsevier, 2018-05) Acosta Rosales, Carina Andrea; López, Clara; Paniagua González, Gema; Garcinuño Martínez, Rosa Mª; Fernández Hernando, Pilar
    Santiago del Estero is a province located in northwestern Argentina. The Dulce River is used for irrigation through a vast network of channels and ditches, including the San Martin Canal (SMC), which crosses the capital city of Santiago del Estero. This canal's water is used for drinking, as well as recreational use for the general population. However, this river has been seriously polluted for several decades. The present study focuses on the identification and the quantification of the water pollution levels of total phenols in the SMC according to the seasonal periods. Water samples from various areas of the canal in different months of the year, extending from December to September, were collected for analysis. Additionally, the concentration of total dissolved solids (TDS), chlorides, sulphates, nitrites and organic matter, as well as water hardness and alkalinity, were analysed in order to conduct a more complete study of the contamination of this area. The results showed a worrying total phenol concentration that exceeded the limit set by Argentine legislation for drinking water, as well as water for recreational use (5 μg/L). The total phenol (TP) concentration was directly determined by a molecular absorption spectroscopy method based on a new flow injection analysis system (FIA). Under the selected experimental conditions, the detection and quantification limits were 0.0490 and 0.1633 μg/mL, respectively. The developed method provides a number of improvements related to the speed of analysis, the restricted consumption of the reagents and sample volumes and the unnecessary sample treatment that contribute to environmentally friendly analytical chemistry. The results showed that TP make a significant contribution in the SMC pollution, especially during the months of April (400 ± 110 μg/L) and September (240 ± 20 μg/L). A high sulphate concentration that was higher than the limit allowed by the legislation was also found.
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    Statistical evaluation of fluoride contamination in groundwater resources of Santiago del Estero Province , Argentina
    (Elsevier, 2020-11) Rondano Gómez, Karina del Valle; López Pasquali, Clara Elena; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    This study investigates the suitability of statistical techniques for evaluating the fluoride content and the groundwater quality from Robles Department (RD) and Banda Department (BD) areas in Santiago del Estero (Argentina). Groundwater mineralization is driven by many processes such as, weathering of volcanic products, geothermal activity and human activities. The original matrix consisted of 9 parameters estimated (fluoride content, pH, conductivity, environmental and water temperatures, total dissolved solids, chloride concentration, hardness and alkalinity) from 110 groundwater samples collected of 23 selected scattered rural areas. Groundwater samples were obtained by sampling in wells at different depths. The fluoride levels were determined by a standard colorimetric method in two seasonal periods, dry (from April to September) and rainy (from October to March). Parameters such as pH and total dissolved solids (TDS) reached their highest values in the rainy season; while the temperature, alkalinity, chloride concentration and hardness did it in the dry season. In both seasons, the environmental temperature average was 22 °C. Regarding the fluoride content, approximately the fifty percent of the analyzed groundwater samples exceeded the upper limit (1.0 mg/L) established by the current legislation, obtaining concentration levels between 0.01-2.80 mg/L. This study demonstrates the usefulness of univariate (quartiles calculation, interquartile range IQR) and multivariate statistical method of principal component analysis (PCA) and clusters to establish a better understanding of the environmental status of the region studied and the degree of pollution.
  • Miniatura
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    Corrigendum to “Occurrence of common plastic additives and contaminants in mussel samples: Validation of analytical method based on matrix solid-phase dispersion”
    (Springer, 2021) Cañadas, Raquel; Garrido Gamarro, Esther; Garcinuño Martínez, Rosa Mª; Paniagua González, Gema; Fernández Hernando, Pilar; https://orcid.org/0000-0002-2935-6655
  • Miniatura
    Publicación
    Determination of atropine and scopolamine in honey using a miniaturized polymer-based solid-phase extraction protocol prior to the analysis by HPLC-MS/MS
    (Elsevier, 2024-04-09) Fernández Pintor, Begoña; Gañán Aceituno, Judith; Morante Zarcero, Sonia; Sierra Alonso, Isabel; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    Two homopolymers have been prepared employing methacrylic acid and 4-vynylpiridine as functional monomers (p-MAA, p-4-VP) through an easy and quick precipitation polymerization method for application as sorbents in solid-phase extraction (SPE) to determine atropine and scopolamine in honey. The optimized SPE conditions were as follows: 25 mg of p-MAA, 4 mL of sample loading volume (diluted honey 1:10 with water), 4 mL of elution solvent (methanol/water with 1 % formic acid, 80/20, v/v). The extracts were analyzed by HPLC-MS/MS. The cartridges were reusable for forty cycles demonstrating an environmentally friendly approach. The methodology was validated in terms of linearity, accuracy, precision, selectivity, matrix effect and sensibility, highlighting the absence of matrix effect. The miniaturized polymer-based SPE was successfully applied to fifteen honeys, showing concentrations up to 7.23 ng/g in the most contaminated honey. All quantified honey samples (5 in total) were of multifloral type.
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    Occurrence of erythromycin residues in sheep milk. Validation of an analytical method
    (Elsevier, 2015-04) Soledad Rodríguez, Beatriz Elena; Durand Alegría, Jesús Senén; García Mayor, M Asunción; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    The paper describes a new and selective analytical sample treatment for quantitative extraction and preconcentration of erythromycin in presence of other macrolide antibiotics in sheep milk samples. The methodology is based on the use of a molecular imprinted polymer (MIP) employed as solid phase extraction sorbent (MISPE). The synthesized material by bulk polymerization using erythromycin (ERY) as template was evaluated as solid phase extraction sorbent, in a novel sample treatment technique that can be coupled to high-performance liquid chromatography with diode-array detector (HPLC-DAD). MIP selectivity was studied for other macrolide antibiotics with similar structures, such as tylosin (TYL), spiramycin (SPI), josamycin (JOS), roxithromycin (ROX) and ivermectin (IVER) getting recoveries for these interferents lower than 35%, for all cases except for ROX, which recoveries were around 85%. The variables affecting the molecularly imprinted solid-phase extraction (MISPE) procedure were optimized to select the best conditions of selectivity and sensitivity to determine ERY at concentration levels established by EU legislation in sheep milk. Under the selected experimental conditions, quantification limit was 24.1 µg kg−1. Recoveries were higher than 98%, with RSDs between 0.7% and 2%. The proposed MISPE-HPLC method was validated and successfully applied to ERY analysis in sheep milk samples.
  • Miniatura
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    Identification and morphological characterization of different types of plastic microparticles
    (Elsevier, 2024-05-15) Soliz Rojas, Dulce Lucy; Paniagua González, Gema; Muñoz Arnanz, Juan; Bravo Yagüe, Juan Carlos; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    The knowledge of the polymeric composition of microplastics (MPs) is interesting because offers useful information on the resistance, durability, and degradability of these materials, also allowing progress in the control of this contamination. However, there is currently a lack of reliable standardized methods for the identification, and characterization of the plastic microparticles. This work uses different techniques in a complementary manner for the identification, and characterization of MPs that more frequently are found in the environment. A total of 10 types of plastics were collected (polystyrene (PS), polyethylene terephthalate (PETE), polyethylene (PE), high- and low-density polyethylene (HDPE and LDPE, respectively), polyvinyl chloride (PVC), polypropylene (PP), polytetrafluoroethylene (PTFE), Polyamide (PA, Nylon 6,6) and poly-carbonate (PC)) and their chemical identification were analyzed by reflectance-attenuated infrared (FTIR-ATR). Furthermore, the samples were observed using light microscopy, and scan-ning electron microscopy (SEM). Also, staining with 12 different dyes was performed to improve the identification of microplastics. The results of this study revealed that PETE, PE, HDPE and LDPE, whose SEM images exhibited smoothness and flat uniformity of their surface, were not (or less) susceptible to adsorb staining solutions while PP, PA, PVC, and PTFE, were capable of adsorbing the dye solutions.
  • Miniatura
    Publicación
    Synthesis and characterization of a molecularly imprinted polymer for the determination of spiramycin in sheep milk
    (Elsevier, 2017-04-15) Durand Alegría, Jesús Senén; García Mayor, M Asunción; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª
    A series of molecularly imprinted polymers (MIPs) comprising reactionary sites which are complementary to macrolide antibiotic spiramycin (SPI) were synthetized by noncovalent bulk polymerization technique. MIPs were synthesized under different polymerization process and their recognition efficiency was evaluated in binding studies in comparison with non-imprinted polymers. The best MIP was morphologically characterized and equilibrium assays were carried out. The MIP was evaluated as a sorbent for extraction and preconcentration of SPI from aqueous and sheep milk samples, and an off-line MISPE method followed by high-performance liquid chromatography with UV diode-array detection was established. Good linearity were obtained for SPI in a range of 24–965 μg kg−1 and the average recoveries at three spiked levels in milk samples were higher than 90% (RSD < 5%). Limit of quantification was 24.1 μg kg−1. Cross-reactivity studies from other macrolides with similar structure were tested. The optimum imprinted polymer showed a good selectivity and affinity for SPI, demonstrating the potential of the proposed MISPE for rapid, sensitive and effective sample pretreatment for selective determination of SPI in sheep milk samples.
  • Miniatura
    Publicación
    Quantification of differential tissue biomarker responses to microplastic ingestion and plasticizer bioaccumulation in aquaculture reared sea bream Sparus aurata
    (Elsevier, 2022-08) Capó Fiol, Xavier; Alomar, Carme; Compa, Monserrat; Solé, Montserrat; Sanahuja, Ignasi; Deudero, Salud; Soliz Rojas, Dulce Lucy; Paniagua González, Gema; Garcinuño Martínez, Rosa Mª; https://orcid.org/0000-0002-3499-5494
    Marine aquaculture is considered a potential source of microplastics (MPs). MPs can induce oxidative stress and damage in marine species. In this study we evaluated the impact of MPs intake in the commercial fish, Sparus aurata , from aquaculture facilities and the antioxidant response associated to this MPs ingestion in caged specimens for 120 days. Sampling was carried out at the beginning of the study T 0 at 60 days (T 60 ) and at 120 days (T 120 ). At each sampling stage, gastrointestinal tract, blood, plasma, liver and muscle samples were obtained to analyse MPs intake (gastrointestinal tract), oxidative stress markers (blood, plasma and liver) and plasticizers bioaccumulation (muscle). Fish sampled at T 60 presented the highest MPs intake and plasticizers accumulated in muscle over time, but with a different pattern according to type: bisphenols and phthalates. This indicates MPs ingestion induces a differential tissue response in S. aurata . Similarly, stress biomarkers presented a differential response throughout the study, depending on the analysed tissue. In the case of oxidative damage markers, for malondialdehyde (MDA) an increase throughout the study was observed both in liver and blood cells but with a progressive decrease in plasma. In the case of phase I detoxifying enzyme activities in liver, 7-ethoxyresorufin O-deethylase (EROD), 7-benzyloxy-4-[trifluoromethyl]coumarin-O-debenzyloxylase (BFCOD) and carboxylesterases (CE), showed a comparable decrease at T 60 with a slight recovery at T 120 . In contrast, glutathione- S -transferase (GST) activity was significantly enhanced at T 60 compared to the other sampling stages. In conclusion, MPs ingestion occurs in aquaculture reared seabream where potentially associated plasticizers accumulate in the muscle and both could be responsible for plasma and liver oxidative stress damage and alterations on detoxifying biomarkers responses